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Potassium Carbonate → HCID 59632933, 화합물

HRID 2369093
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HRID 2369093 반응식
Br[C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:12]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[Cl:19])[N:11]=[C:10]([C:20]([O:22][CH3:23])=[O:21])[CH:9]=2)=[N:6][CH:7]=1.[CH3:24][S:25]([C:28]1[CH:29]=[C:30](B(O)O)[CH:31]=[CH:32][CH:33]=1)(=[O:27])=[O:26].C([O-])([O-])=O.[K+].[K+]>COCCOC.CCOC(C)=O.O.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[Cl:19][C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=1[N:12]1[C:8]([C:5]2[CH:4]=[CH:3][C:2]([C:32]3[CH:31]=[CH:30][CH:29]=[C:28]([S:25]([CH3:24])(=[O:27])=[O:26])[CH:33]=3)=[CH:7][N:6]=2)=[CH:9][C:10]([C:20]([O:22][CH3:23])=[O:21])=[N:11]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 3

HCID 11430Potassium CarbonateHCID 27735423-(Methylsulfonyl)phenylboronic acidHCID 59632248HCID 59632248, 화합물

생성물 1

HCID 59632933HCID 59632933, 화합물

시약·촉매·용매 4

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)촉매
HCID 962
Water
용매
HCID 80711,2-Dimethoxyethane용매
HCID 8857Ethyl Acetate용매

반응 조건

온도
120 °C

실험 절차

Methyl 5-(5-bromopyridin-2-yl)-1-(2-chlorophenyl)-1H-pyrazole-3-carboxylate (200 mg, 0.51 mmol), 3-(methylsulfonyl)phenylboronic acid (120 mg, 0.60 mmol) and dichloro[1,1′-bis(diphenylphosphino)ferrocene]palladium (11) dichloromethane adduct (20 mg, 24 μmol), and K2CO3 (0.45 mL of a 3.5M aqueous solution, 1.6 mmol) were combined in DME (2.5 mL) in a microwave reaction vessel. The dark mixture was heated at 120° C. for 5 minutes. The reaction mixture was diluted with EtOAc and H2O. The aqueous layer was removed and extracted with additional EtOAc. The combined organics were dried over Na2SO4, treated with some decolorizing carbon and filtered through a pad of Celite. Concentration of the filtrates under reduced pressure and purification by flash column chromatography eluting with 0% to 50% MeCN/CH2Cl2 afforded methyl 1-(2-chlorophenyl)-5-(5-(3-(methylsulfonyl)phenyl)pyridin-2-yl)-1H-pyrazole-3-carboxylate as a pale yellow foam. This material was carried on to the subsequent step. MS(ES): 468 [M+H]+.

후처리

  1. customThe aqueous layer was removed
  2. extractionextracted with additional EtOAc
  3. dry with materialThe combined organics were dried over Na2SO4
  4. additiontreated with some decolorizing carbon
  5. filtrationfiltered through a pad of Celite
  6. customConcentration of the filtrates under reduced pressure and purification by flash column chromatography
  7. washeluting with 0% to 50% MeCN/CH2Cl2

출처 및 근거

ORD 기록
ord-76a2f60fb5214ddaad7c364b20e295fe
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08703805B2

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